A sulfur-containing polyimide precursor has been modified by the homog
eneous addition of tris(2,4-pentanedionato)iron(III) or tris(1-phenyl-
2,4-pentanedionato)iron(III). The synthesis of the resulting free-stan
ding film of iron-modified polyimide via thermal condensation is also
described. It was observed that the presence of iron promoted the oxid
ation of the thioether moiety in the polyimide backbone as determined
by X-ray photoelectron spectroscopy (XPS) and reflectance Fourier tran
sform infrared spectroscopy (FT-IR). The effect of cure atmosphere on
the oxidation of the sulfur, the thermal properties of the composite,
and the distribution of iron oxide particles within the free-standing
film are also examined.